CN102001706B - Method for producing bismuth oxide by pyrogenic process - Google Patents
Method for producing bismuth oxide by pyrogenic process Download PDFInfo
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- CN102001706B CN102001706B CN201010548257A CN201010548257A CN102001706B CN 102001706 B CN102001706 B CN 102001706B CN 201010548257 A CN201010548257 A CN 201010548257A CN 201010548257 A CN201010548257 A CN 201010548257A CN 102001706 B CN102001706 B CN 102001706B
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Abstract
The invention discloses a method for producing bismuth oxide by a pyrogenic process. The method comprises the following steps of: crushing a bismuth ingot into powder, sieving the powder, adding the powder into a horizontal rotary oxidation furnace, raising the temperature, controlling the temperature of the oxidation furnace in a step-by-step heating way, wherein the step-by-step heating comprises repeated temperature rise stage and temperature-consistent stage, at the same time, introducing oxygen to oxidize the bismuth powder, after the oxidization stage is finished, stopping introducing oxygen, reducing the temperature to the room temperature and taking out the powder to obtain the bismuth oxide. Compared with the prior art, the method adopts the rotary furnace to achieve the effect of 'stirring'. The step-by-step temperature rise and temperature control measure contributes to full contact and oxidation reaction between the bismuth in various phase states and under different active degrees and the oxygen; and the reaction efficiency and the yield are effectively guaranteed.
Description
Technical field
The present invention relates to a kind of working method of pyrogenic process bismuth oxide.
Background technology
The chemical formula Bi of bismuth oxide (Bismuth oxide)
2O
3, molecular weight 465.96,820 ℃ of fusing points, 1890 ℃ of boiling points, specific density (water=1) 8.5.Bismuth oxide is yellow heavy powder or monoclinic crystal, and odorlessness is stable in the air, and heating becomes maroon and still becomes yellow after cold.Bismuth oxide is dissolved in hydrochloric acid and nitric acid; Water-soluble hardly.Bi
20
3Be used to prepare mineral dye, high dioptric glass, glass is used in nuclear engineering, and magneticsubstance also can be used as organic catalyst, electroplating additive, medicinal astringent matter, fire-retardant for plastic, glass-ceramic tinting material.Bi particularly
20
3As a kind of electronic functional material, be widely used in voltage dependent resistor, zinc oxide lightning rod device, CTT, the manufacturing of electronic industrial products such as electrical condenser.In addition, in battery industry and the superconductor technology Bi is arranged also
20
3Application.
In bismuth series product industrial chain, the production of the high quality bismuth oxide ring that is absolutely necessary, the production technique of bismuth oxide is divided into bismuth salt calcination method, bismuth metal direct oxidation method and bismuth-containing material facture in the world.
Summary of the invention
The problem that the present invention need solve is the working method with a kind of pyrogenic process bismuth oxide that is the basis with the bismuth metal direct oxidation method; This method guarantees the reactivity of reaction process through the temperature control mode of ladder heating; The heating of this ladder comprise heat up with the constant temperature stage repeat to occur (down with), make bismuth meal and oxygen in horizontal oxidized still, react the formation bismuth oxide.
Having designed a kind of working method of pyrogenic process bismuth oxide according to the above-mentioned problem that solves, is raw material with bismuth meal and oxygen, accomplishes bismuth meal and the reaction process of oxygen in horizontal oxidized still through the mode of ladder temperature control, and the step of this method is following:
(1) bismuth ingot is broken, powder process and sieving obtains 10~600 purpose bismuth meals;
(2) bismuth meal that 150~400kg is sieved drops in the horizontal oxidized still, loads onto the two ends fire door;
(3) in temperature-rise period, through ladder temperature control mode heated oxide stove, while aerating oxygen oxidation bismuth meal;
(4) oxidation stage finishes, and stops oxygen supply and cooling;
(5) after temperature is reduced to room temperature, come out of the stove, obtain bismuth oxide;
(6) bismuth oxide obtains satisfactory bismuth oxide after sieving.
Wherein, bismuth ingot is the 5N bismuth ingot of purity 99.999%; The oxygen flow that feeds in the step (3) is 1~5m
3/ h, oxygen purity are 2N~4N, and the speed with 80~100 ℃/hour heats up in the step (3), and difference constant temperature is 2~8,2~8,3~5,1~4,2~6 hours under 250,350,450,550,650 ℃.Described oxidized still is converter, rotation when the temperature rise period begins, and rotation frequency is 3~10Hz; And in temperature-rise period, described oxidized still rotates in the temperature-fall period, and in step (4) temperature-fall period, stops the oxidized still rotation when cooling to 200~300 ℃.
Because the fusing point very low (271.3 ℃) of bismuth, if too fast in the starting stage heating, the bismuth with elementary that does not react with oxygen will oxidized bismuth parcel, causes oxidizing reaction incomplete; In reaction (production) process, the fused bismuth also may flow out body of heater, causes the difficulty of coming out of the stove; In the reaction process, the transitional form of the mutual parcel that bismuth and bismuth oxide form can effectively stop the fusing of unreacted bismuth meal, so in entire reaction course, answer strict controlled temperature; At high temperature, bismuth and oxygen reaction are violent, discharge a large amount of heat, must in reaction process, strictness control oxygen flow.Thus; The present invention compared with prior art; Adopt rotary oven to reach the effect of " stirring ", be beneficial to bismuth through the ladder temperature control mode and under each phase and different active degree, contact with oxygen fully and carry out oxidizing reaction, guaranteed reaction efficiency and yield rate effectively.
Description of drawings
Accompanying drawing 1 is the schematic flow sheet of pyrogenic process bismuth oxide working method of the present invention.
Embodiment
Purport of the present invention is to solve the problem that reaction is incomplete, product yield is low that exists in the bismuth metal direct oxidation method.So, by rotary oven the raw material in the reaction is carried out " stirrings ", and be aided with stage intensification and constant temperature temperature control, bismuth is contacted with oxygen under each phase and different active degree fully and carry out oxidizing reaction.Below in conjunction with accompanying drawing the present invention is made further detailed description.
The horizontal rotation oxidized still that uses among the present invention is autonomous design and manufacturing, and agent structure comprises base, and base is provided with BOGEY WHEEL; Body of heater is shelved on the BOGEY WHEEL; BOGEY WHEEL makes the body of heater rotation through being connected with transmission shaft, variator and motor and the motivating force of motor being passed to body of heater, is provided with fire door at the two ends of body of heater, and a fire door is provided with oxygen intake; Another fire door is provided with oxygen outlet, on body of heater, adds heating jacket.
It is raw material that the present invention is still with bismuth meal (the 5N bismuth ingot with purity 99.999% makes), and directly (oxygen purity is the reaction generation bismuth oxide of 2N~4N) with oxygen in oxidized still.
With reference to accompanying drawing.The step of the inventive method is:
(1) bismuth ingot is broken, powder process and sieving obtains 10~600 purpose bismuth meals;
(2) bismuth meal that 150~400kg is sieved drops in the horizontal oxidized still, loads onto the two ends fire door;
(3) in temperature-rise period, through ladder-elevating temperature and temperature control heated oxide stove, while aerating oxygen (oxygen purity is 2N~4N, down together) oxidation bismuth meal;
(4) oxidation stage finishes, and stops oxygen supply and cooling;
(5) after temperature is reduced to room temperature, come out of the stove, obtain bismuth oxide;
(6) bismuth oxide obtains satisfactory bismuth oxide after sieving.
Wherein, the oxygen flow that feeds in the step (3) is 1~5m
3/ h, and the speed with 80~100 ℃/hour heats up in the step (3), and difference constant temperature is 2~8,2~8,3~5,1~4,2~6 hours under 250,350,450,550,650 ℃.Described oxidized still is converter, rotation when the temperature rise period begins, and rotation frequency is 3~10Hz; And in temperature-rise period, described oxidized still rotates in the temperature-fall period, and in step (4) temperature-fall period, stops oxidized still when cooling to 200~300 ℃ and revolve rotation.
According to said step, enumerating following specific embodiment is reference.
Embodiment 1
The method that a kind of pyrogenic process bismuth oxide is produced, operation is following:
(1) the 5N bismuth ingot is broken, powder process and sieving obtains 600 purpose bismuth meals.
(2) bismuth meal that 200kg is sieved drops in the horizontal oxidized still, loads onto the two ends fire door.
(3) start rotating machine, the oxidized still rotation frequency is 4Hz; Open heating system, heat up with 80~100 ℃/hour speed, difference constant temperature is 3,5,4,2,2 hours under 250,350,450,550,650 ℃; At 200 ℃ of beginning aerating oxygens, flow is 1m
3/ h.
(4) oxidation stage finishes, and motor stops the rotation when cooling to 200~300 ℃.
(5) after temperature is reduced to room temperature, come out of the stove, obtain bismuth oxide.
(6) bismuth oxide obtains the bismuth oxide that is of the required size after sieving.
Embodiment 2
The technology that a kind of pyrogenic process bismuth oxide is produced comprises following operation:
(1) the 5N bismuth ingot is broken, powder process and sieving obtains 200 purpose bismuth meals.
(2) bismuth meal that 350kg is sieved drops in the horizontal oxidized still, loads onto the two ends fire door.
(3) start rotating machine, the oxidized still rotation frequency is 9Hz; Open heating system, heat up with 80~100 ℃/hour speed, difference constant temperature is 7,4,4,3,5 hours under 250,350,450,550,650 ℃; At 200 ℃ of beginning aerating oxygens, flow is 5m
3/ h.
(4) oxidation stage finishes, and motor stops the rotation when cooling to 200~300 ℃.
(5) after temperature is reduced to room temperature, come out of the stove, obtain bismuth oxide.
(6) bismuth oxide obtains the bismuth oxide that is of the required size after sieving.
Embodiment 3
The method that a kind of pyrogenic process bismuth oxide is produced, operation is following:
(1) the 5N bismuth ingot is broken, powder process and sieving obtains 400 purpose bismuth meals.
(2) bismuth meal that 400kg is sieved drops in the horizontal oxidized still, loads onto the two ends fire door.
(3) start rotating machine, the oxidized still rotation frequency is 7Hz; Open heating system, heat up with 80~100 ℃/hour speed, difference constant temperature is 6,7,3,2,3 hours under 250,350,450,550,650 ℃; At 200 ℃ of beginning aerating oxygens, flow is 2m
3/ h.
(4) oxidation stage finishes, and stops oxygen supply when cooling to 200~300 ℃, and motor stops the rotation.
(5) after temperature is reduced to room temperature, come out of the stove, obtain bismuth oxide.
(6) bismuth oxide obtains the bismuth oxide that is of the required size after sieving.
Embodiment 4
The method that a kind of pyrogenic process bismuth oxide is produced, operation is following:
(1) the 5N bismuth ingot is broken, powder process and sieving obtains 100 purpose bismuth meals.
(2) bismuth meal that 350kg is sieved drops in the horizontal oxidized still, loads onto the two ends fire door.
(3) start rotating machine, the oxidized still rotation frequency is 6Hz; Open heating system, heat up with 80~100 ℃/hour speed, difference constant temperature is 8,7,4,4,2 hours under 250,350,450,550,650 ℃; At 200 ℃ of beginning aerating oxygens, flow is 2.5m
3/ h.
(4) oxidation stage finishes, and stops oxygen supply when cooling to 200~300 ℃, and motor stops the rotation.
(5) after temperature is reduced to room temperature, come out of the stove, obtain bismuth oxide.
(6) bismuth oxide obtains the bismuth oxide that is of the required size after sieving.
Embodiment 5
The method that a kind of pyrogenic process bismuth oxide is produced, operation is following:
(1) the 5N bismuth ingot is broken, powder process and sieving obtains 10 purpose bismuth meals.
(2) bismuth meal that 370kg is sieved drops in the horizontal oxidized still, loads onto the two ends fire door.
(3) start rotating machine, the oxidized still rotation frequency is 8Hz; Open heating system, heat up with 80~100 ℃/hour speed, difference constant temperature is 8,8,4,3,3 hours under 250,350,450,550,650 ℃; At 200 ℃ of beginning aerating oxygens, flow is 3m
3/ h.
(4) oxidation stage finishes, and stops oxygen supply when cooling to 200~300 ℃, and motor stops the rotation.
(5) after temperature is reduced to room temperature, come out of the stove, obtain bismuth oxide.
(6) bismuth oxide obtains the bismuth oxide that is of the required size after sieving.
Can know that by above-mentioned instance when the order number of bismuth meal was low, the constant temperature soaking time behind ladder-elevating temperature was just longer, so that reaction fully, so do not advise adopting the low mesh number bismuth meal generally speaking.Disclosed embodiment only is used for explaining treatment process of the present invention more than the event, and the equivalent variations of doing according to the disclosure of invention still belongs to the invention protection domain.
Claims (6)
1. a pyrogenic process bismuth oxide working method is a raw material with bismuth meal and oxygen, accomplishes bismuth meal and the reaction process of oxygen in horizontal oxidized still through the mode of ladder-elevating temperature and temperature control, and the step of this method is following:
(1) bismuth ingot is broken, powder process and sieving obtains 10~600 purpose bismuth meals;
(2) bismuth meal that 150~400kg is sieved drops in the horizontal oxidized still, loads onto the two ends fire door;
(3) in temperature-rise period, through ladder-elevating temperature and temperature control heated oxide stove, while aerating oxygen oxidation bismuth meal;
(4) oxidation stage finishes, and stops oxygen supply and cooling;
(5) after temperature is reduced to room temperature, come out of the stove, obtain bismuth oxide;
(6) bismuth oxide obtains satisfactory bismuth oxide after sieving;
Described step (3) heats up with 80~100 ℃/hour speed, and difference constant temperature is 2~8,2~8,3~5,1~4,2~6 hours under 250,350,450,550,650 ℃.
2. pyrogenic process bismuth oxide working method according to claim 1 is characterized in that: described bismuth ingot is the 5N bismuth ingot of purity 99.999%.
3. pyrogenic process bismuth oxide working method according to claim 2 is characterized in that: the oxygen flow that feeds in the said step (3) is 1~5m
3/ h, oxygen purity are 2N~4N.
4. according to claim 1 or 2 or 3 described pyrogenic process bismuth oxide working methods, it is characterized in that: oxidized still is converter, and rotation frequency is 3~10Hz.
5. pyrogenic process bismuth oxide working method according to claim 4 is characterized in that: in temperature-rise period, described oxidized still begins rotation in temperature-fall period.
6. pyrogenic process bismuth oxide working method according to claim 5 is characterized in that: in step (4) temperature-fall period, stop the oxidized still rotation when cooling to 200~300 ℃.
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RU2478080C2 (en) * | 2011-05-20 | 2013-03-27 | Федеральное государственное бюджетное учреждение науки Институт неорганической химии им. А.В. Николаева Сибирского отделения Российской академии наук (ИНХ СО РАН) | Method of producing powdered bismuth (iii) oxide |
RU2474537C2 (en) * | 2011-05-20 | 2013-02-10 | Федеральное государственное бюджетное учреждение науки Институт неорганической химии им. А.В. Николаева Сибирского отделения Российской академии наук (ИНХ СО РАН) | Method of producing powdered bismuth (iii) oxide |
RU2478081C2 (en) * | 2011-05-20 | 2013-03-27 | Федеральное государственное бюджетное учреждение науки Институт неорганической химии им А.В. Николаева Сибирского отделения Российской академии наук (ИНХ СО РАН) | Method of producing powdered bismuth (iii) oxide |
CN103184384B (en) * | 2013-03-12 | 2015-12-09 | 宁波汉博贵金属合金有限公司 | A kind of preparation method of Composite silver stannic oxide electric contact material |
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US20040115121A1 (en) * | 2002-12-13 | 2004-06-17 | Clark Manufacturing, LLC. | Method for making oxide compounds |
CN101687664A (en) * | 2007-04-25 | 2010-03-31 | 丹石产业株式会社 | The method and the equipment used thereof that prepare bismuth oxide |
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US20040115121A1 (en) * | 2002-12-13 | 2004-06-17 | Clark Manufacturing, LLC. | Method for making oxide compounds |
CN101687664A (en) * | 2007-04-25 | 2010-03-31 | 丹石产业株式会社 | The method and the equipment used thereof that prepare bismuth oxide |
Non-Patent Citations (2)
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